Nishiwaki Akinori, Watanabe Aya, Higashi Kenjirou, Tozuka Yuichi, Moribe Kunikazu, Yamamoto Keiji
Graduate School of Pharmaceutical Sciences, Chiba University, 1-33 Yayoi-cho, Inage-ku, Chiba 263-8522, Japan.
Int J Pharm. 2009 Aug 13;378(1-2):17-22. doi: 10.1016/j.ijpharm.2009.05.023. Epub 2009 May 22.
Modes of molecular interaction between prednisolone and mesoporous materials have been investigated by the technique of solid-state NMR. Folded sheet mesoporous material (FSM-16) was used as host material and prednisolone was used as guest molecule. A suspension of FSM-16 in prednisolone dichloromethane solution was evaporated to prepare the evaporated samples. (13)C NMR spectroscopy was used as well as powder X-ray diffractometry and differential scanning calorimetry. Crystalline behavior of prednisolone disappeared in the evaporated samples, indicating the monomolecular dispersion of prednisolone in FSM-16 matrices. NMR peak shifts and broadening could be attributed to the molecular interaction between the A ring of prednisolone and FSM-16. Thermal properties of prednisolone were investigated after heat treatment of the evaporated samples. The results indicated that the thermal stability of the dispersion made from FSM-16 of large pore size was superior to that from FSM-16 of small pore size. Hydrocortisone was used to compare the dispersion state with prednisolone. It was suggested that the double bond at the C-1 and C-2 positions of prednisolone might play an important role in the process of adsorption of prednisolone to FSM-16.
通过固态核磁共振技术研究了泼尼松龙与介孔材料之间的分子相互作用模式。采用折叠片层介孔材料(FSM - 16)作为主体材料,泼尼松龙作为客体分子。将FSM - 16悬浮于泼尼松龙二氯甲烷溶液中蒸发以制备蒸发样品。使用了(13)C核磁共振光谱以及粉末X射线衍射法和差示扫描量热法。在蒸发样品中泼尼松龙的结晶行为消失,表明泼尼松龙在FSM - 16基质中呈单分子分散。核磁共振峰的位移和展宽可归因于泼尼松龙的A环与FSM - 16之间的分子相互作用。对蒸发样品进行热处理后研究了泼尼松龙的热性质。结果表明,大孔径FSM - 16制成的分散体的热稳定性优于小孔径FSM - 16制成的分散体。使用氢化可的松来比较其与泼尼松龙的分散状态。研究表明,泼尼松龙C - 1和C - 2位的双键可能在泼尼松龙吸附到FSM - 16的过程中起重要作用。